CN106086944A - A kind of method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect - Google Patents
A kind of method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect Download PDFInfo
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- CN106086944A CN106086944A CN201610534242.8A CN201610534242A CN106086944A CN 106086944 A CN106086944 A CN 106086944A CN 201610534242 A CN201610534242 A CN 201610534242A CN 106086944 A CN106086944 A CN 106086944A
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- layer
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- superoleophobic
- metal substrate
- method preparing
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2506/00—Halogenated polymers
- B05D2506/10—Fluorinated polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2518/00—Other type of polymers
- B05D2518/10—Silicon-containing polymers
Abstract
The invention discloses a kind of method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect, use the composite electroformed technique under suitable pulse electrical quantity to be more easy to obtain fine and close smooth compound cast layer；The structure with different concave curvature can be obtained by selecting different polymer size, change degree of swelling and moulding pressure, thus obtain the surface of the work that oleophobic property is controlled；The technology and equipment that this invention uses is simple, with low cost, it is adaptable to the superoleophobic modification in large-area metal surface.
Description
Technical field
The present invention relates to a kind of method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect, be used for changing metal
Surface wettability so that it is there is superoleophobic characteristic.Being applicable to the preparation on the superoleophobic surface of large area, preparation cost is low, easily realizes,
Belong to field of electrochemical deposition.
Background technology
Moistening (Wetting) is that solid interface is changed into the phenomenon of solid-liquid interface by solid-air interface.And wettability
(wettability) ability or tendentiousness that a kind of liquid sprawls at a kind of surface of solids are referred to.Wettability is to there is nature
In universal phenomenon, such as rainwater fall to being formed spherical drop after lotus leaf surface and the phenomenon that tumbles and Folium Nelumbinis " go out mud and
Do not contaminate " self_cleaning effect, be super-hydrophobic phenomenon.In addition the many foot of animals and plants such as water skipper, the wing of butterfly, Rice Leafs
Deng, it may have ultra-hydrophobicity.Research shows, the superhydrophobic characteristic that all these surfaces are had is due to micro-nano coarse knot
Structure and low-surface energy substance cooperatively form.
Wettability is also material science and the importance in Surface Engineering field simultaneously, in daily life, commercial production, agriculture
Industry has many important application in producing.So-called super-hydrophobic refer to the water droplet static contact angle at the surface of solids more than 150 °, in like manner,
Superoleophobic is that the oil droplet static contact angle at the surface of solids is more than 150 °.But, the surface tension of oil droplet is much smaller than the table of water droplet
Surface tension, therefore, preparation has the surface of solids of superoleophobic characteristic, and its difficulty is bigger than super hydrophobic surface, it more difficult to realize.Phase
Pass research shows, in air to be prepared, superoleophobic surface is in addition to needing the modification of low-surface-energy molecule, also will be at its band micro-nano
Rice introduces concave surface curvature on coarse structure surface so that micro-nano coarse structure is indent or cantilever-shaped.This gives and manufactures work
Skill proposes bigger challenge.
At present, substantial amounts of document is it has been reported that artificial bionic super hydrophobic surface, and these materials are at self-cleaning surface, anti-
Ice, antifog, anti-pollution, anticorrosion, fluid drag-reduction is widely used.Report about oleophobic surface is relatively fewer, but super
Oleophobic surface is such as grease proofness coating in industrial and agricultural production, the antifouling process of sea water, and petroleum pipeline is grease proofing creeps, in oil-water separation
There is huge application space.Metal material is widely applied in engineering, uses face extremely extensive, but the antipollution of metal is prevented
Corrosive nature is poor, and therefore on metal, preparation has superoleophobic characteristic surface and is significant.
So-called surface texture (Surface texture) refers to that body surface has certain size and the pit of arrangement, recessed
The array of the pattern such as trace or convex closure.Have the surface of micro-nano-scale microcosmic texture surface energy, optical characteristics, bionical characteristic,
The aspects such as mechanical property, hydrodynamic characteristics and friction and wear behavior and smooth surface show distinct feature, this
It is filled with new vitality for numerous disciplinary study, and shows huge application potential at many engineering fields.
The preparation method of oleophobic surface is generally followed from bottom to top or top-to-bottom method.Existing prepare superoleophobic surface
Process substantially have following several: (1) without template wet etching (2) femtosecond laser etching method (3) method of electrostatic spinning (4) electricity
Sedimentation (5) sol-gel process etc..
Prior art is primarily present following shortcoming: (1) can etch silicon and polymer surfaces, efficiency without template wet etching
High cost is low, but etching surface morphology controllable is poor, and this method is readily obtained super hydrophobic surface, but is difficult to obtain superoleophobic surface.
Oleophobic surface can be obtained by Bosch etching method, but complex process, with high costs；(2) femtosecond laser etching method can be prepared
Precision is high, the micro-nano nested structure surface of pattern rule, but this process efficiency is low, is not suitable for manufacturing on a large scale, and equipment is extremely
Expensive；(3) method of electrostatic spinning is by utilizing micro-/ nano filament at surface construction coarse structure, large area can prepare super-hydrophobic material
Material, but the controllability of the super hydrophobic material surface micro-structure prepared and uniformity are poor, wear no resistance, and service life is relatively
Short；(4) common electrodeposition process can deposit metal or polymer, can prepare the most easily and have micro-nano coarse structure table
Face, but pattern randomness is strong, wayward, and it is not likely to produce the secondary groove structure of indent or cantilever.
Summary of the invention
For the shortcoming of above-mentioned prior art, it is an object of the invention to propose one and prepare Metal Substrate based on swelling effect
The method of superoleophobic compound cast layer, is the improvement of conventional electrodeposition method, can produce the indent of morphology controllable or the secondary of cantilever
Groove structure.
According to an aspect of the present invention, a kind of side preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect is proposed
Method: the metallic substrates through deoiling is connected power supply as electroforming negative electrode, nickel plate as anode by (1), at anode and negative electrode
Between pass to Dispersed precipitate have polymeric material microparticle ball Ni-based electroforming solution constitute electroforming system.Energising makes in electroforming solution
The Ni-based disperse that polymer micropellet ball and nickel ion are about 50～80um at metal substrate surface codeposition formation thickness is combined
Electroformed layer；(2) deposition has after electro-deposition completes the metallic substrates of electroformed layer be electrolysed as anode, removes electroformed layer surface
Upper one layer of very thin nickel metal so that the polymer micropellet ball of the Dispersed precipitate revealed self is as micro-bulge structure；
(3) height of surface of the work micro-bulge is milled to basically identical by the workpiece precision grinder through Electrolyzed Processing；(4) by dimpling
The body partial inversion away from its top about 1/3 height immerses swelling softening in alcohol solution and applies with one piece of smooth flat pressing plate 9
Pressure (1000Pa < P < 5000Pa) be pressed in micro-bulge surface make its soften part produce irreversible deformation, obtain after deformation
Micro nano structure is the secondary groove structure of indent or cantilever.(5) finally the carrying tablet of silicon fluoride is had jointly to put with dripping workpiece
Carry out toasting in hermetic container and make silicon fluoride pass through the adsorption low-surface-energy at surface of the work one layer of nano thin-layer of formation
Material, finally makes metal surface reach superoleophobic performance.
According to an aspect of the present invention, the material of microparticle ball is polymeric material, and being immersed in alcohol solution can be swelling
Soften, but will not dissolve；Swelling period carry out speed is not only relevant with temperature, and with the molecular weight of high polymer and
Change degree is relevant, also the most relevant with solvent.
According to an aspect of the present invention, the selection of microparticle ball must be consistent with particle diameter (20～30um), and it is at electroformed layer
Middle volume fraction controls in the range of 40～60%, and the spacing that the too small meeting of volume fraction makes particle sphere be distributed is excessive, volume fraction
Cross conference and affect the formation of cast layer.Particle diameter and the volume fraction of appropriate mix are so that forming indent or cantilever in subsequent handling
Secondary groove structure.
According to an aspect of the present invention, after the micro-bulge after swelling softening is pressurizeed by smooth flat pressing plate, Jing Guoyi
The pressurize fixed time can produce irreversible deformation.
According to an aspect of the present invention, in step (1), the metallic substrates smooth to surfacing can be with filling ethanol
The ultrasonic washing unit of solution is carried out, and recycles removal of surfactant oxidation on metal surface layer, finally uses deionized water
Cleaning is placed in baking oven drying removes surface moisture.
According to an aspect of the present invention, in step (2), electroforming solution adds appropriate surfactant, it
Can adsorb in large quantities micro-nano particle ball surface formed one layer of firm adsorbed film.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention；
Fig. 2 is indent or the secondary groove structure figure of cantilever of the present invention.
Detailed description of the invention
Embodiments of the invention are described below in detail, and the example of described embodiment is shown in the drawings, the most from start to finish
Same or like label represents the element of same or like function.The embodiment described below with reference to accompanying drawing is to show
Example, it is only used for explaining the present invention, and is not considered as limiting the invention.On the contrary, embodiments of the invention include falling
Enter all changes, amendment and the equivalent in the range of the spirit of attached claims and intension.
Such as Fig. 1, a kind of to prepare the method flow of the superoleophobic compound cast layer of Metal Substrate based on swelling effect as follows:
S1, the pre-treatment of metallic substrates 1: after metallic substrates 1 is soaked oil removing with hot alkaline solution, with acetone and deionized water
Rinse further, be placed at 120 DEG C of vacuum drying oven dehydration 15min, to go the removal of impurity to make texture be connected jail with metallic substrates 1
Gu.
S2, metallic substrates 1 surface dispersion are composite electroformed: use nickel plate 2 as anode, metallic substrates 1 as negative electrode, both
Being connected respectively to positive pole and the negative pole of power supply 5, passing to Dispersed precipitate between the anode and cathode has the microparticle of polymeric material
The Ni-based electroforming solution 4 of ball 3, thus constitute electroforming system.Negative electrode generation reduction reaction after energising, makes polymer in electroforming solution 4 micro-
Granule ball 3 and nickel ion form, at metallic substrates 1 surface codeposition, the Ni-based disperse composite electroforming deposit that thickness is about 50～80um
6；
In this step, electrical quantity: electric current density 0.5～5A/dm2Square-wave pulse, frequency 0.5～3KHz, dutycycle
20～80%, process time (depending on cast layer thickness) etc.；Formulation of electroforming solution: Ni (CH2SO3)2·4H2O 200～500g/L,
NiCl2·6H2O 15～30g/L, H3BO330～45g/L, pH value about 4, temperature about 50 DEG C etc..
S3, the electrolysis of Ni-based disperse composite electroforming deposit: electro-deposition complete after by the anode and cathode reversal connection of electroforming system, make deposition
The metallic substrates 1 having electroformed layer 6 is electrolysed as anode.Anode generation oxidation reaction after energising, removes on electroformed layer 6 surface
One layer of very thin nickel metal so that the polymer micropellet ball 3 of the Dispersed precipitate revealed self is as micro-bulge 7.
In this step, by controlling electrical quantity: electric current density 10～15A/dm2Unidirectional current, process time (according to remove
Thickness is fixed) control the removal thickness (about particle sphere radius size) of nickel metal layer.Removal thickness is crossed conference and is caused particle sphere easy
Come off in cast layer, remove thickness too small, be not easily formed the needed micro-bulge of subsequent handling 7.
S4, polish micro-bulge: cleaned up by the workpiece taking-up deionized water through Electrolyzed Processing, will with precision grinder
The height of surface of the work micro-bulge 7 is milled to basically identical, then cleans up with deionized water and dry up with nitrogen.
S5, swelling softening: under constant temperature and pressure (25～65 DEG C, P0), (can basis away from its top about 1/3 height by micro-bulge 7
Need to adjust) partial inversion immerse in alcohol solution 8, make to be soaked part and suck the abundant swelling softening of alcohol solution 8.
S6, pressurizing and deformation: the workpiece after abundant swelling softening is taken out, applies pressure with one piece of smooth flat pressing plate 9
(1000Pa < P < 5000Pa) be pressed in micro-bulge 7 surface make its soften part produce irreversible deformation, the micro-nano obtained after deformation
Rice structure is the secondary groove structure 10 of indent or cantilever.Pressurize certain time makes structure 10 curing molding, then separates pressing plate 9
Take out workpiece.
S7, low-surface-energy are modified: by through the workpiece of Electrolyzed Processing with drip that to have the carrying tablet of silicon fluoride 11 to be collectively disposed at close
Close in container, be then placed in 65 DEG C of baking ovens and toast 1 hour, put after taking-up to room temperature, complete the preparation of workpiece.In baking process
In, silicon fluoride 11, by being formed the low-surface energy substance of one layer of nano thin-layer at surface of the work by adsorption, makes metal surface
Reach superoleophobic performance.
The workpiece finally prepared is as shown in Figure 2.
More preferably, in step sl, can be clear with the ultrasound wave filling ethanol solution to the metallic substrates 1 that surfacing is smooth
Washing machine is carried out, and recycles removal of surfactant oxidation on metal surface layer, finally cleans with deionized water and be placed in baking oven
Middle drying removes surface moisture.Make metallic substrates 1 surface cleaning clean free from admixture non-oxidation layer, it is simple to deposit on its surface
Metal level and metallic substrates have stronger adhesion.
More preferably, in step s 2, adding appropriate surfactant in electroforming solution, they can adsorb in large quantities
Micro-nano particle ball surface forms one layer of firm adsorbed film, can effectively prevent micro-nano particle from reuniting and being aided with super in electroforming system
Acoustic or electrical magnetic vibration is stirred, and more can promote particle suspension effect than simple mechanical type stirring.
Compared with prior art, advantages of the present invention has: 1) use the compound electric foundry work under suitable pulse electrical quantity
Skill is more easy to obtain fine and close smooth compound cast layer；2) can by select different polymer size, change degree of swelling and
Moulding pressure obtains the structure with different concave curvature, thus obtains the surface of the work that oleophobic property is controlled；3) this invention makes
Technology and equipment simple, with low cost, it is adaptable to the superoleophobic modification in large-area metal surface.
In the case of spiritual without departing from the present invention or necessary characteristic, the present invention can be embodied in other specific forms.Should
Described specific embodiment each side is considered merely as illustrative and non-limiting.Therefore, scope of the invention such as appended claims
Scope is shown rather than shown as indicated above.All fall change in the equivalent meaning and scope of claim should be regarded as
Fall in the category of claim.
Claims (6)
1. the method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect, it is characterised in that comprise the following steps:
(1) metallic substrates through deoiling is connected power supply as electroforming negative electrode, nickel plate as anode, between the anode and cathode
Passing to the Ni-based electroforming solution composition electroforming system that Dispersed precipitate has the microparticle ball of polymeric material, energising makes to be polymerized in electroforming solution
Thing microparticle ball and nickel ion form, at metal substrate surface codeposition, the Ni-based disperse composite electroforming deposit that thickness is 50～80um；
(2) deposition has after electro-deposition completes the metallic substrates of electroformed layer be electrolysed as anode, removes on electroformed layer surface very thin
One layer of nickel metal so that the polymer micropellet ball of the Dispersed precipitate revealed self is as micro-bulge structure；(3) will be through
The height of surface of the work micro-bulge is milled to basically identical by the workpiece precision grinder crossing Electrolyzed Processing；(4) by micro-bulge away from it
The partial inversion of top about 1/3 height immerses swelling softening in alcohol solution and applies pressure pressure with one piece of smooth flat pressing plate 9 again
Making on micro-bulge surface it soften part and produce irreversible deformation, wherein pressure size is 1000Pa < P < 5000Pa, after deformation
The micro nano structure obtained is the secondary groove structure of indent or cantilever；(5) finally by workpiece with drip and have the carrying tablet of silicon fluoride
It is collectively disposed in hermetic container to carry out toasting and makes silicon fluoride pass through adsorption to form the low of one layer of nano thin-layer at surface of the work
Surface energy substance, finally makes metal surface reach superoleophobic performance.
2. the method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect as claimed in claim 1, it is characterised in that
The material of described microparticle ball is polymeric material.
3. the method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect as claimed in claim 1, it is characterised in that
The selection of described microparticle ball must be consistent with particle diameter, and its size is 20～30um, and its volume fraction in electroformed layer controls
In the range of 40～60%.
4. the method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect as claimed in claim 1, it is characterised in that
Being pressurizeed the micro-bulge after swelling softening by smooth flat pressing plate, the pressurize through certain time can produce irreversible change
Shape.
5. the method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect as claimed in claim 1, it is characterised in that
In step (1), the metallic substrates smooth to surfacing can be carried out with the ultrasonic washing unit filling ethanol solution, then
Utilize removal of surfactant oxidation on metal surface layer, finally clean with deionized water to be placed in baking oven drying and remove surface water
Point.
6. the method preparing the superoleophobic compound cast layer of Metal Substrate based on swelling effect as claimed in claim 1, it is characterised in that
In step (2), adding appropriate surfactant in electroforming solution, they can adsorb in large quantities on micro-nano particle ball surface
Form one layer of firm adsorbed film.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610534242.8A CN106086944B (en) | 2016-07-07 | 2016-07-07 | A kind of method that the superoleophobic compound cast layer of Metal Substrate is prepared based on swelling effect |
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| CN201610534242.8A CN106086944B (en) | 2016-07-07 | 2016-07-07 | A kind of method that the superoleophobic compound cast layer of Metal Substrate is prepared based on swelling effect |
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| CN106086944B CN106086944B (en) | 2018-06-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112606442A (en) * | 2020-11-25 | 2021-04-06 | 绍兴上虞明吉塑业有限公司 | Treatment process for preventing liquid from being easily stained on suction head |
| US11380604B2 (en) | 2019-11-26 | 2022-07-05 | Toyota Motor Engineering & Manufacturing North America, Inc. | Methods of forming electronic assemblies with textured surfaces using low current density electroplating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11380604B2 (en) | 2019-11-26 | 2022-07-05 | Toyota Motor Engineering & Manufacturing North America, Inc. | Methods of forming electronic assemblies with textured surfaces using low current density electroplating |
| CN112606442A (en) * | 2020-11-25 | 2021-04-06 | 绍兴上虞明吉塑业有限公司 | Treatment process for preventing liquid from being easily stained on suction head |
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|---|---|
| CN106086944B (en) | 2018-06-12 |
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